Study of uranium contamination of ground water in Punjab state in India using X-ray fluorescence technique

The elemental concentration of uranium in the samples collected from the ground water and the canal water in the Bathinda district of Punjab state, India, have been investigated using X-ray fluorescence technique. The residues obtained after drying the water samples were analysed using the energy dispersive X-ray fluorescence spectrometer consisting of Mo-anode X-ray tube equipped with selective absorbers as an excitation source and an Si(Li) detector. The uranium concentration values in significant fraction of the shallow ground water samples from the hand pumps is found to be above the permissible level of 15?ppb recommended by World Health Organisation for the drinking water, and its values in the canal water samples are below 5?ppb. To investigate the flyash from the coal-fired thermal power plants as a possible source of ground water contamination, the water samples collected from the surroundings of the power plants and the flyash samples were also analyzed. The results rule out flyash as a source of uranium contamination. Agrochemical processes occurring in the calcareous soils in the region are the favoured potential source of uranium contamination of the ground water.     

Neutron diffraction characterization of Japanese artworks of Tokugawa age

Neutron time-of-flight diffraction technique has been used to characterize some Japanese historical artifacts. With this method, metal samples can be analyzed in their bulk properties without need of sampling. Results shown here were obtained at the Italian Neutron Experimental Station (INES@ISIS) located at the pulsed neutron source ISIS (UK). The parallel use of a scanning electron microscope equipped with an energy-dispersive X-ray fluorescence device (SEM-EDX) permitted a full quantitative characterization of the investigated samples, namely four hand-guards (Tsubas) of Japanese swords attributed to the Tokugawa age. In particular, we were able to obtain, in a totally non-invasive non-destructive way, a full quantitative phase characterization of the samples, a detailed Bragg peak broadening analysis, and a quantitative texture determination. These results, complemented with those obtained via the traditional analysis method of SEM-EDX, allowed a full characterization of both the bulk and the surface of the artifacts.     

有机非线性光学晶体NPP的AFM研究

有机二阶非线性光学活性晶体的分子设计和晶体工程是复杂而又引人注目的课题．有机非线性光学晶体N一忡硝基苯基）－LWe脯氨醇（NPP）是一个极为成功的自］子山．由于在＊＊P分子中引入了含手性碳原子和可形成分子间氢键的电子给体脯氨醇，使得其分子跃迁偶极矩与单科P21晶体结构的二重轴之间的夹角为586”．接近于理论优化值（54．74”），因此，＊＊P具有很高的宏观二阶非线性光学活性，其粉末二次谐波强度为尿素的150倍．自1984年首次报导以来，对它的晶体生长门和物理性质已进行了广泛深入的研究．原子力显微镜（＊＊M）能够以极高…     

Improved instrumental sensitivity for Cd determination in aqueous solutions using Wavelength Dispersive X-ray Fluorescence Spectrometry,Rh-target tube instrumentation

This work was aimed at improving the instrumental sensitivity and detection limits for Cd determination in liquid samples by using conventional Wavelength Dispersive X-ray Fluorescence (WDXRF) instrumentation equipped with Rh-anode X-ray sources.     

Analytical characterization of municipal solid waste incinerator fly ash

The synergy of the micro FT-IR (Fourier Transform-Infrared) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-ray) techniques has been shown to be particularly helpful and effective for the characterization of inorganic compounds in fly ashes. The experimental data obtained by these techniques have been interpreted in comparison with those of other techniques. The presence of calcium carbonate, some sulfates, ammonium nitrate, calcium hydrogen phosphate, some chlorides, some oxides and aluminium silicates have been verified.     

Analytical characterization of municipal solid waste incinerator fly ash. Part II

The synergy of the micro FT-IR (Fourier Transform-Infrared) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-ray) techniques has been shown to be particularly helpful and effective for the characterization of inorganic compounds in fly ashes. The experimental data obtained by these techniques have been interpreted in comparison with those of other techniques. The presence of calcium carbonate, some sulfates, ammonium nitrate, calcium hydrogen phosphate, some chlorides, some oxides and aluminium silicates have been verified.     

Elemental concentrations and source identification of air particulate matter at a Nigerian site: A preliminary study

Air particulate matter collected between July and October 1990 at a site located close to an industrial estate in Lagos, Nigeria were analyzed for 18 elements by Wavelength Dispersive X-ray Fluorescence Spectroscopy (XRF) and Atomic Absorption Spectroscopy (AAS). Varimax rotated factor analysis was used for source identification of the coarse and fine fractions. For the coarse fraction, the major sources are: Re-entrained soil, Sea-salt, Industry, Regional sulphate and fresh automobile exhaust. For the fine fraction, the sources identified are Re-entrained soil, Vehicle exhaust, Sea-salt, and Industrial processes. Two other sources which are likely to be due to specific industrues come out in the fine fraction but they have not been clearly identified.     

In situ Hochdruck- und Hochtemperatur-Untersuchungen an Siliciumsuboxiden mittels energiedispersiver Röntgenbeugung

In situ High-Pressure- and High-Temperature Studies of Siliconsuboxides via Energy Dispersive X-ray Diffraction The amorphous silicon compounds Si₂O₃, H₂Si₂O₄, HSiO_1.5, and SiO have been investigated under High-Pressure- and High-Temperature conditions in situ via energy dispersive X-ray diffraction with synchrotron radiation. The studies have been performed using the Multi Anvil High Pressure Device MAX-80, at HASYLAB, DESY-Hamburg, Germany. Except for SiO, at a pre-set pressure of 45 kbars the formation of Coesite was observed at heating. Commercially available SiO did not crystallize in any way, indicating that it seems not to consist of silicon(II)-oxide, but is in fact a mixture of silicon and silicondioxide, disproportionated on an atomic scale.     

X射线晶体学结合电子晶体学在复杂无机晶体结构解析中的应用

自然界中的材料,比如无机材料,有机材料,生物材料等等,均有其独特的物理和化学性质。而材料的性能又与材料的结构息息相关,只有充分了解了材料的结构,才能更加深入的研究材料性质。因此,材料结构的确定在化学、物理、生物等学科中的显得尤为重要。X射线晶体学作为传统的结构解析技术仍然是目前最重要的结构解析手段,但是对于复杂结构,X射线衍射晶体学解析结构也存在一些不足,往往需要其他技术手段相补充才能完成复杂结构的结构解析。电子晶体学虽然起步比X射线晶体学晚,但是,经过近几十年的发展,已经是结构解析领域一个非常重要的手段。本文将主要介绍X射线晶体学结合电子晶体学在复杂无机晶体结构解析中的应用。     

金属组学：高通量分析技术进展与展望

金属组学是系统研究一种细胞、组织或完整生物体内全部金属原子的分布、含量、化学种态及其功能的新兴综合学科,它的提出受到人们越来越多的关注。本文综述了金属组学的研究方法,并对各种方法的特点和局限性做了比较说明．ICP-MS与NAA技术可实现多元素同时定量分析,同步辐射微束CT及μRF,EDX,PIXE,SIMS及LA-ICP—MS亦可实现金属组分布研究．金属组学研究目前正处于发展初期,仍有许多困难特别是分析仪器及方法方面的问题有待解决．已有的金属组形态及结构分析工作大多数采用的是较低效率的分析方法,一些正在发展中的关键技术平台,如HTXAS可真正实现高通量的形态或结构分析．此外,生物信息学有望成为金属组学研究的重要工具之一．     

Expression, Purification, Crystallization and Molecular Replacement Studies of TorI, an Inhibition Protein of Tor System

TorI, a Tor system inhibitor acting through protein-protein interaction with the TorR response regulator, is an excisionase that interacts with the integrase and DNA during prophage excision. It has been crystallized by the vapor-diffusion method using polyethylene glycol 3350 as a precipitant at pH 8.5. The X-ray diffraction data sets from the TorI crystal was collected at a resolution of 2.1 , using a synchrotron source. The crystal belongs to primitive monoclinic lattice with cell parameters of 46.210 × 53.992 × 73.561     

Experimental and theoretical charge density study of chemical bonding in a Co dimer complex

The charge density of Co2(CO)6(HC[triple bond]CC6H10OH) (1) in the crystalline state has been determined using multipolar refinement of single-crystal X-ray diffraction data collected (i) with a synchrotron source at very low temperatures (15 K) and (ii) using a conventional source with the crystal at intermediate temperature (100 K). The X-ray charge density model is augmented by complete active space and density functional theory calculations. Topological analyses of the different charge distributions show that the two Co atoms are not bonded to each other in the quantum theory of atoms in molecules (QTAIM) sense of the word. However, the behavior of the source function and the total energy density indicate that there is some bond-like character in the Co-Co interaction. The bridging alkyne fragment provides an unusual bonding situation, with extremely small electron density differences between the two Co-C bond critical points and the "CoC2" ring critical point. Thus, the structure is close to a topological catastrophe point. Comparison of the results obtained from the two diffraction data sets and ab initio theory suggests that the topology of the experimental electron density in this special atomic environment is highly sensitive to subtle effects of measurement errors and potential shortcomings of the multipole model, or to effects of the crystal field. Thus, even the two identical molecules in the asymmetric unit show altered bonding patterns.     

Preparation of bismuth telluride thin film by electrochemical atomic layer epitaxy (ECALE)

Thin-layer electrochemical studies of the underpotential deposition (UPD) of Bi and Te on cold rolled silver substrate have been performed. The voltammetric analysis of underpotential shift demonstrates that the initial Te UPD on Bi-covered Ag and Bi UPD on Te-covered Ag fitted UPD dynamics mechanism. A thin film of bismuth telluride was formed by alternately depositing Te and Bi via an automated flow deposition system. X-ray diffraction indicated the deposits of Bi₂Te₃. Energy Dispersive X-ray Detector quantitative analysis gave a 2: 3 stoichiometric ratio of Bi to Te, which was consistent with X-ray Diffraction results. Electron probe microanalysis of the deposits showed a network structure that results from the surface defects of the cold rolled Ag substrate and the lattice mismatch between substrate and deposit. Translated from Chinese Journal of Applied Chemistry, 2005, 22 (11) (in Chinese)     

Carbon-supported manganese for heterogeneous activation of peroxymonosulfate for the decomposition of phenol in aqueous solutions

Phenolic substances are harmful to humans and other living things, even at low concentrations. Therefore, phenol must be removed from water with the proper process. One of the most effective processes for degrading phenol is heterogeneous catalytic oxidation. Three carbon materials as supports were used to prepare manganese-oxide based catalyst (2.5% MnOx/ACP and 2.5% MnOx/ACN), and graphene oxide (2.5% MnOx/GO). These catalysts were tested for the degradation of phenol in aqueous solution using peroxymonosulfate as a source of sulfate radical. The physio-chemical catalysts were characterised by several characterisation techniques such as powder X-ray diffraction, N₂-sorption (BET), scanning electron microscopy (SEM) equipped with Dispersive Energy X-ray Spectroscopy (EDS). In comparison to other catalysts, heterogeneous activation of peroxymonosulfate was more effectively done by 2.5% MnOx/ACP, resulting in a higher production rate of sulfate radicals. In the presence of a catalyst at 0.2 g and 1 g peroxymonosulfate in 500 mL solution at 25 °C, 90% total organic carbon (TOC) removal and phenol decomposition of 100% was achieved in 90 min with phenol concentration of 75 mg/L. First-order kinetics were followed by phenol decomposition with the energy of activation on 2.5% MnOx/ACP of 15.0 kJ/mol.     

Preparation and crystal structure of Ba2NF

Single crystalline Ba₂NF was prepared by heating a mixture of KCuF₃ and Ba metal to 900°C under dynamic flow of N₂, followed by slow cooling from the melt. Crystals of Ba₂NF were dark violet in color and very air sensitive. X-ray diffraction experiments revealed that Ba₂NF is isostructural with rocksalt-type BaO, and has space group Fm-3 m (No. 225) with cell parameter of , Z=2. X-ray data was collected on a Bruker SMART APEX 4k CCD Single Crystal Diffractometer at 100 K, using Mo(K_α) radiation. Structure refinement was carried out by full-matrix least squares on F² on all data, to give R₁=0.0194 (all data) and wR₂=0.0433 for 3 parameters and 23 independent reflections. The final position assignments were analyzed via bond valence sum calculations.     

XPS and TOF-SIMS applied to the study of ancient artifacts: Further studies on Alexandrian tetradrachms from the time of the Julio-Claudian dynasty

Two tetradrachms from the Diniacopoulos collection housed at Queen's University are the subject of this study. Previously, a protocol had been developed for a coin of the Emperor Claudius from the same collection, which showed that a combination of Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS), Energy Dispersive X-ray Spectroscopy (EDX), and X-ray Photoelectron Spectroscopy (XPS) could provide information and identify areas of interest for additional analysis, thereby minimizing the amount of damage incurred. This is now applied to two more tetradrachms issued by the same mint and dated respectively to the time of Tiberius (14–37 AD) and Nero (54–68 AD). Preliminary results have indicated both differences and similarities between these coins and that from the time of Claudius. By comparing these results, it is hoped that information as to how the coins were made can be elucidated, shedding light on the different components and composition of the alloys produced in the same mint but at different time periods. Moreover, the detection and the identification of corrosion products, along with understanding what restorations methods may have been applied in the past, can guide conservators to determine what conservation treatment and preservation strategies are most appropriate for these antiquities.     

Beyond crystallography: the study of disorder, nanocrystallinity and crystallographically challenged materials with pair distribution functions

Studying the structure of disordered and partially ordered materials is notoriously difficult. Recently, significant advances have been made using the atomic pair distribution function (PDF) analysis of powder diffraction data coupled with the use of advanced X-ray and neutron sources and fast computers. Here we summarize some of the more spectacular successes of this technique in studying the structure of complex materials and compounds. Our purpose is to make the PDF analysis technique familiar to the chemical community by describing its methodologies and highlighting its potential in solving structural characterization problems that are intractable by any other technique available to this community e.g. single crystal diffraction, Rietveld refinement of powder diffraction data and extended X-ray absorption fine structure analysis (EXAFS).     

The application of x-ray diffraction analysis to uranium ceramics: Quantitative analysis of the binary mixture UO2-U3O8

An X-ray diffraction method is proposed for the quantitative analysis of the binary mixture UO₂—U₃O₈. Diffractometer and Debye-Scherrer camera techniques were compared ; the former is preferable whenever sufficient sample is available. The relative standard deviation was found to be 1%.     

D8X射线衍射仪简易变温加热台的研制

成功研制的简易变温加热台,在不更换D8X射线衍射仪的附件情况下,能快速方便的安装在衍射仪上,进行X射线衍射原位变温测试,满足了从室温至600℃的原位变温X射线衍射测试需求.更换附件时间从2~3天缩短至30 min即可进行变温X射线衍射测试,提高了测试效率.同时,节省了购买同类变温加热台近20万元的资金.     

Syntheses，Structures and Properties of Some New Composition Perovskite Compounds：Sr_（0．6）Bi_（0．4）FeO_（2．7），Sr_（1－x）Bi_xFeO_（3－y） and Ba_（1．5）Pt_（0．5）Mn_2O_6

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